CN112323016A - Ceramic metal sputtering film forming process - Google Patents
Ceramic metal sputtering film forming process Download PDFInfo
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- CN112323016A CN112323016A CN202011267536.1A CN202011267536A CN112323016A CN 112323016 A CN112323016 A CN 112323016A CN 202011267536 A CN202011267536 A CN 202011267536A CN 112323016 A CN112323016 A CN 112323016A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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Abstract
The invention discloses a ceramic metal sputtering film-forming process, which comprises the following steps of carrying out integral process processing on a ceramic body, a metal film body, an electroplated nickel layer, other additives and the like according to the basic type of the ceramic metal sputtering film-forming process, wherein the process basic processing comprises carrying out integral process processing on the ceramic body, the metal film body, the electroplated nickel layer and other additives, the ceramic body is ground, the ultrasonic processing is adopted, the external surface of the ceramic body is firstly subjected to sputtering covering processing, the subsequent silver firing processing and the silver firing processing are simple and easy to operate, the ceramic body after silver firing can be more uniform, bubbles on the surface of a silver layer after high-temperature sintering can be inhibited, the surface of the silver layer is smooth and flat, the problems of poor tension, scalding of the silver layer, non-bright surface and the like can be avoided, compared with common ceramics, the sintered ceramic body is more stable, has better, the ceramic body has high density and high air tightness after being sealed.
Description
Technical Field
The invention relates to the technical field of metal sputtering film formation, in particular to a ceramic metal sputtering film formation process.
Background
Ceramic substrate metallization includes vapor deposition metallization methods such as vacuum evaporation, vacuum sputtering, ion plating, and the like, which are increasingly widely used in recent years. The sputtering process is divided into two-stage sputtering, four-stage sputtering, advanced sputtering and the like, wherein direct current two-sister sputtering is the simplest and is also the substrate form of the sputtering process. Firstly, a vacuum container is in high vacuum, argon gas with certain pressure is filled, then direct current negative high voltage (1-7 kv) is applied to a cathode sputtering target which is at a certain distance from a ceramic support stage (at ground potential), and glow discharge is caused. And (4) bombarding positive ions and negative ions of the discharge gas to a target with negative high pressure, and depositing the hard metal on the ceramic to form a metallized film. Typically, the first layer of metal is sputter deposited as molybdenum, tungsten, niobium, vanadium, etc., followed by a layer of a metal such as gold, silver, palladium, platinum, or copper that is easily wetted by the solder. It is naturally also possible to electroplate a nickel or copper layer on the first sputtered layer. Firstly, vacuumizing the system to 6.7 times 10-GPa, closing a valve of a diffusion pump, filling pure argon into the system through the valve until the pressure is (1-4 times 10-1 Pa. tungsten cathode is heated, and maintaining the inside of a cylinder with the diameter of about 8-10 cm for 15-20 min to form argon discharge, 5 times 10-3The T magnetic field enables the plasma region to be limited in a cylinder with the diameter of 8-10 cm per month, the plasma region is maintained for 15-20 min, plasma is formed, the ceramic surface is scrubbed, and the preheating effect is achieved. The sputtering target is subjected to a negative high pressure. Sputtering was done for 5min with the shutter plate and then the shutter plate was removed to allow the target metal to sputter directly onto the ceramic to the desired thickness. And the surface of the workpiece is bombarded by ions by adopting high-frequency ionized argon, the requirement on the negative high voltage of the target is lower at the moment, the target is generally 1-3 kv, and the sputtering time is 3-5 min. A vacuum tight seal is required for the first metal layer sputtered onto the ceramic part, then the sputtered second metal is dissolved in the first metal and easily wetted by the solder, the first layer can be very thin, but the second layer needs to be thick enough (1um) to prevent the solder from dissolving the second layer. However, the conventional method of sputtering a metal plating film involves many small bubbles on the surface of the metal plating film when the operation is not proper, and thus the sputtering quality is lowered and many defective products are produced. Therefore, the invention provides a ceramic metal sputtering film-forming process so as toThe problems set forth in the above background art are solved.
Disclosure of Invention
The present invention is directed to a sputtering deposition process for ceramic metal, which solves the above problems of the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a ceramic metal sputtering film-forming process comprises the following steps:
step S1: according to the basic type of the ceramic metal sputtering film-forming process, the process basic processing comprises the integral processing of a ceramic body, a metal film body, an electroplated nickel layer, other additives and the like;
step S2: pretreating, namely cleaning the ceramic body integrally;
step S3: coating a silver layer, namely putting the smooth and clean ceramic body into a sputtering machine, wherein the metal raw material added in the sputtering machine is conductive silver paste;
step S4: silver drying, namely placing the ceramic body subjected to sputtering processing by a sputtering machine in a silver drying furnace for processing;
step S5: silver is burnt, and the ceramic body after silver drying is calcined again;
step S6: electroplating a nickel layer;
step S7: cooling;
as a further scheme of the present invention, step S2 specifically includes:
polishing the sintered ceramic body, then carrying out ultrasonic cleaning to remove residual grinding agents and stains on the surface, and drying the cleaned ceramic body at the drying temperature of 150-300 ℃ to obtain a smooth and clean ceramic body;
as a further scheme of the present invention, step S3 specifically includes:
uniformly sputtering and coating conductive silver paste on the surface of the porcelain by using a sputtering machine, selecting a proper scraper according to the preset silver film thickness to scrape and brush the conductive silver paste on the surface of the porcelain body, and uniformly coating the conductive silver paste on the surface of the porcelain so as to achieve sputtering of a metal layer;
as a further scheme of the present invention, step S4 specifically includes:
the ceramic piece coated with the silver paste is dried in a silver drying furnace, the silver drying temperature is about 120 ℃, the silver drying furnace is most suitable, and the silver drying furnace has the function of volatilizing other components in the silver paste before the product is placed into high-temperature sintering, so that small holes in the silver paste can be naturally compounded, bubbles on the surface of the silver layer after high-temperature sintering can be inhibited, and the surface of the silver layer is smooth and flat;
as a further scheme of the present invention, step S5 specifically includes:
sending the ceramic piece after silver baking into a silver baking furnace for silver baking, forming a metal film body on the surface of the ceramic body, wherein the peak temperature is 750-850 ℃, glass powder and ethyl cellulose are melted in the silver baking process, so that the metal film body is more uniformly attached to the ceramic body, the sintering furnace has the function of completely solidifying the silver paste, and the sintering process parameter value needs temperature treatment, otherwise, the stability of the silver layer can be influenced, the problems of poor tension, scalding of the silver layer, non-bright surface and the like can be avoided;
as a further scheme of the present invention, step S6 specifically includes: nickel is electroplated on the surface of the metal film body 2 to achieve the nickel electroplating layer, so that the silver layer can be prevented from being oxidized, and the silver layer is protected;
as a further scheme of the present invention, step S7 specifically includes:
and standing the processed ceramic body 1 for 1-2 hours, and storing or performing subsequent processing after the ceramic body is completely cooled.
As a further proposal of the invention, the ceramic metal film is prepared by the preparation method, and the average strength of the ceramic metal film exceeds 330 MPa.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the ceramic body is ground, the processing is improved by adopting ultrasonic processing, the outer surface of the ceramic body is sputtered and covered, then the metal film body is integrally dried by the silver baking furnace to prepare the metal film, the raw material control and operation are simpler, the subsequent silver baking processing and the operation are simple and easy, the ceramic body after silver baking can be more uniform, the bubbles on the surface of the silver layer after high-temperature sintering can be inhibited, the surface of the silver layer is smooth and flat, the problems of poor tension, scald on the silver layer, non-bright surface and the like can be avoided, compared with common ceramics, the sintered ceramic body is more stable and better in quality, the vent holes can be well filled, the distribution is uniform and continuous, the density of the ceramic body is high, and the air tightness after sealing is high.
Drawings
FIG. 1 is a schematic structural diagram of a sputtering deposition process for ceramic metal.
FIG. 2 is a schematic structural diagram of steps in a sputtering deposition process for ceramic metal.
In the figure: 1. a ceramic body; 2. a metal film body; 3. and electroplating a nickel layer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-2, in an embodiment of the invention, a ceramic metal sputtering film forming process includes the following steps:
step S1: according to the basic type of the ceramic metal sputtering film-forming process, the process is processed, and the process comprises the steps of integrally processing a ceramic body 1, a metal film body 2, an electroplated nickel layer 3, other additives and the like;
step S2: pretreating, namely firstly cleaning the ceramic body 1 integrally, specifically, polishing the sintered ceramic body 1, then ultrasonically cleaning to remove residual grinding agents and stains on the surface, and drying the cleaned ceramic body 1 at the drying temperature of 150-300 ℃ to obtain a smooth and clean ceramic body 1;
step S3: coating a silver layer, namely putting the smooth and clean ceramic body 1 into a sputtering machine, wherein the metal raw material added in the sputtering machine is conductive silver paste, and specifically, uniformly sputtering and coating the conductive silver paste on the surface of a ceramic piece through the sputtering machine, and selecting a proper scraper to scrape and brush the conductive silver paste on the surface of the ceramic body 1 according to the preset silver film thickness so as to uniformly coat the conductive silver paste on the surface of the ceramic piece, thereby achieving the purpose of sputtering a metal layer;
step S4: baking silver, namely placing the ceramic body 1 which is sputtered and processed by a sputtering machine in a silver baking furnace for processing, specifically, baking a ceramic piece coated with the silver paste in the silver baking furnace, wherein the silver baking temperature is about 120 ℃, which is most suitable, and the silver baking furnace has the function of volatilizing other components in the silver paste before the product is placed in high-temperature sintering, so that small holes in the silver paste can be naturally compounded, bubbles on the surface of the silver layer after the high-temperature sintering can be inhibited, and the surface of the silver layer is smooth and flat;
step S5: burning silver, namely burning the ceramic body 1 after silver drying again, specifically, sending the ceramic piece after silver drying into a silver burning furnace for silver burning, forming a metal film body 2 on the surface of the ceramic body 1, wherein the peak temperature is 750-850 ℃, glass powder and ethyl cellulose are melted in the silver burning process, so that the metal film body 2 is more uniformly attached to the ceramic body 1, the silver paste can be completely solidified by the sintering furnace, temperature treatment is required for the numerical value of the sintering process parameter, otherwise, the stability of the silver layer can be influenced, the problems of poor tension, scalding of the silver layer, non-bright surface and the like can be avoided;
step S6: the nickel layer 3 is electroplated, nickel is electroplated on the surface of the metal film body 2, the nickel layer 3 is electroplated, the silver layer can be prevented from being oxidized, and the silver layer is protected;
step S7: and (4) cooling, wherein the processed ceramic body 1 is kept stand for 1-2 hours, and the ceramic body 1 can be stored or processed subsequently after being completely cooled.
The ceramic metal film is prepared by the preparation method, and the average strength of the ceramic metal film is over 330 MPa.
The working principle of the invention is as follows:
according to the invention, the ceramic body 1 is ground, improved and processed by adopting ultrasonic processing, the outer surface of the ceramic body 1 is sputtered and covered, then the metal film body 2 is integrally dried by a silver baking furnace to prepare the metal film, the raw material control and operation are simpler, the subsequent silver baking processing and the operation are simple and easy, the silver-baked ceramic body 1 can be more uniform, the bubbles on the surface of the silver layer after high-temperature sintering can be inhibited, the surface of the silver layer is smooth and flat, the problems of poor tension, scalding of the silver layer, non-bright surface and the like can be avoided, compared with common ceramic, the sintered ceramic body 1 is more stable and better in quality, the exhaust holes can be well filled, the distribution is uniform and continuous, the ceramic body 1 is high in density and the air tightness after sealing is high.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (2)
1. A ceramic metal sputtering film-forming process is characterized in that:
which comprises the following steps:
step S1: according to the basic type of the ceramic metal sputtering film-forming process, the process basic processing comprises the integral processing of a ceramic body, a metal film body, an electroplated nickel layer, other additives and the like;
step S2: the method comprises the following steps of (1) preprocessing, firstly, integrally cleaning a ceramic body, specifically, polishing the sintered ceramic body, then carrying out ultrasonic cleaning to remove residual grinding agents and stains on the surface, and drying the cleaned ceramic body at the drying temperature of 150-300 ℃ to obtain a smooth and clean ceramic body;
step S3: coating a silver layer, namely putting a smooth and clean ceramic body into a sputtering machine, wherein the metal raw material added in the sputtering machine is conductive silver paste, and specifically, uniformly sputtering and coating the conductive silver paste on the surface of a ceramic piece through the sputtering machine, and selecting a proper scraper to scrape and brush the conductive silver paste on the surface of the ceramic body according to the preset silver film thickness so as to uniformly coat the conductive silver paste on the surface of the ceramic piece, thereby achieving the purpose of sputtering a metal layer;
step S4: drying silver, namely placing the ceramic body subjected to sputtering processing by a sputtering machine in a silver drying furnace for processing, specifically, drying a ceramic piece coated with the silver paste in the silver drying furnace, wherein the silver drying temperature is about 120 ℃, and the silver drying furnace has the function of volatilizing other components in the silver paste before the product is placed in high-temperature sintering, so that small holes in the silver paste can be naturally compounded, bubbles on the surface of the silver layer after high-temperature sintering can be inhibited, and the surface of the silver layer is smooth and flat;
step S5: burning silver, and burning the ceramic body after silver baking, specifically, sending the ceramic piece after silver baking into a silver burning furnace for silver burning, forming a metal film body on the surface of the ceramic body, wherein the peak temperature is 750-850 ℃, glass powder and ethyl cellulose are melted in the silver burning process, so that the metal film body 2 is more uniformly attached to the ceramic body, the sintering furnace has the function of completely solidifying silver paste, and the temperature treatment is required for the numerical value of the sintering process parameter, otherwise, the stability of the silver layer can be influenced, and the problems of poor tension, scalding of the silver layer, non-bright surface and the like can be avoided;
step S6: nickel layer electroplating, wherein nickel is electroplated on the surface of the metal film body to achieve nickel layer electroplating, so that the silver layer can be prevented from being oxidized, and the silver layer is protected;
step S7: and cooling, namely standing the processed ceramic body for 1-2 hours, and storing or performing subsequent processing after the ceramic body is completely cooled.
2. The process of claim 1, wherein the average strength of the ceramic metal film is over 330 Mpa.
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| CN202011267536.1A CN112323016A (en) | 2020-11-13 | 2020-11-13 | Ceramic metal sputtering film forming process |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102664055A (en) * | 2012-04-11 | 2012-09-12 | 深圳市大富科技股份有限公司 | Conductive silver paste, method for preparing same and surface metallization method for microwave dielectric ceramics |
| CN106747675A (en) * | 2016-11-29 | 2017-05-31 | 浙江大学 | A kind of method of microwave-medium ceramics surface metalation |
| CN108777200A (en) * | 2018-05-30 | 2018-11-09 | 苏州求是真空电子有限公司 | A kind of preparation method of high-power sensitive ceramic electrode |
| CN111733418A (en) * | 2020-06-30 | 2020-10-02 | 苏州蓝晶研材料科技有限公司 | Ceramic conductive material containing alloy layer and preparation method thereof |
-
2020
- 2020-11-13 CN CN202011267536.1A patent/CN112323016A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102664055A (en) * | 2012-04-11 | 2012-09-12 | 深圳市大富科技股份有限公司 | Conductive silver paste, method for preparing same and surface metallization method for microwave dielectric ceramics |
| CN106747675A (en) * | 2016-11-29 | 2017-05-31 | 浙江大学 | A kind of method of microwave-medium ceramics surface metalation |
| CN108777200A (en) * | 2018-05-30 | 2018-11-09 | 苏州求是真空电子有限公司 | A kind of preparation method of high-power sensitive ceramic electrode |
| CN111733418A (en) * | 2020-06-30 | 2020-10-02 | 苏州蓝晶研材料科技有限公司 | Ceramic conductive material containing alloy layer and preparation method thereof |
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